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WO2019188736A1 - Élément de gradation comprenant un film de verre - Google Patents

Élément de gradation comprenant un film de verre Download PDF

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Publication number
WO2019188736A1
WO2019188736A1 PCT/JP2019/011955 JP2019011955W WO2019188736A1 WO 2019188736 A1 WO2019188736 A1 WO 2019188736A1 JP 2019011955 W JP2019011955 W JP 2019011955W WO 2019188736 A1 WO2019188736 A1 WO 2019188736A1
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WO
WIPO (PCT)
Prior art keywords
layer
light control
film
thickness
glass
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2019/011955
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English (en)
Japanese (ja)
Inventor
晶子 杉野
健太 渡辺
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nitto Denko Corp
Original Assignee
Nitto Denko Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nitto Denko Corp filed Critical Nitto Denko Corp
Priority to CN201980021085.2A priority Critical patent/CN111902769B/zh
Priority to EP19775974.9A priority patent/EP3779577B1/fr
Priority to JP2020509930A priority patent/JP7274458B2/ja
Priority to KR1020207026079A priority patent/KR102865558B1/ko
Priority to US16/979,633 priority patent/US11143892B2/en
Publication of WO2019188736A1 publication Critical patent/WO2019188736A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect
    • G02F1/153—Constructional details
    • G02F1/1533—Constructional details structural features not otherwise provided for
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/29—Laminated material
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/133305—Flexible substrates, e.g. plastics, organic film
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • G02F1/133368—Cells having two substrates with different characteristics, e.g. different thickness or material
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F2202/00—Materials and properties
    • G02F2202/28—Adhesive materials or arrangements

Definitions

  • the present invention relates to a light control element including a glass film.
  • dimming elements have been used as window glass and interior materials for buildings and vehicles. Particularly in recent years, demand and expectation for dimming elements are increasing from the viewpoints of reducing the heating / cooling load, reducing the lighting load, and improving comfort.
  • the light control element uses a liquid crystal material or an electrochromic material, and an electric field driving method for controlling the light transmittance by applying an electric field; a thermochromic method in which the light transmittance varies depending on the temperature; A gas chromic method for controlling the transmittance has been developed.
  • These light control elements are used, for example, as light control glass in which a light control layer is sandwiched between two glass plates.
  • a technique has been proposed in which a light control film in which a light control layer is sandwiched between two resin films is attached to a glass surface (Patent Document 1).
  • the light control glass in which the light control layer is sandwiched between the two glass plates is very heavy and complicated to construct.
  • the light control film like patent document 1 is reduced in weight, there exists a problem that a surface is easy to be damaged and a film deteriorates with time.
  • the present invention has been made to solve the above-mentioned problems, and its main object is to provide a light control device that is lightweight and highly reliable and can be easily attached to a glass surface or the like. is there.
  • a light control device comprising a glass film, a light control layer, a resin film, and an adhesive layer in this order and having a bending radius of 20 mm to 100 mm.
  • the glass film has a thickness of 50 ⁇ m to 200 ⁇ m.
  • the resin film has a thickness of 20 ⁇ m to 200 ⁇ m, and the resin film has an elastic modulus at 23 ° C. of 2 GPa to 10 GPa.
  • the pressure-sensitive adhesive layer has a thickness of 20 ⁇ m to 200 ⁇ m, and the pressure-sensitive adhesive layer has an elastic modulus at 23 ° C. of 1 ⁇ 10 ⁇ 5 GPa to 1 ⁇ 10 ⁇ 2 GPa.
  • the thickness from the glass film to the pressure-sensitive adhesive layer of the light control element is 70 ⁇ m to 500 ⁇ m. According to still another aspect of the present invention, it has a long glass film and a light control layer laminated on one side of the glass film, and the thickness of the glass film is 50 ⁇ m to 200 ⁇ m. A glass film roll with a light control layer is provided.
  • one of the two substrates sandwiching the light control layer is a glass film having a predetermined thickness, and the pressure-sensitive adhesive layer is provided outside the other substrate.
  • the “elongate shape” means an elongated shape having a sufficiently long length with respect to the width, for example, an elongated shape having a length of 10 times or more, preferably 20 times or more with respect to the width. Includes shape.
  • the light control element of this invention is equipped with a glass film, a light control layer, a resin film, and an adhesive layer in this order.
  • the substrate to be bonded to the glass surface or the like is a resin film
  • the other is a thin glass film, so that the exposed surface of the light control element is scratch resistant and resistant. It is possible to achieve weight reduction while providing reliability such as impact properties.
  • the light control element of this invention has flexibility, it can be wound in roll shape, Furthermore, since it is lightweight and is equipped with an adhesive layer, it can be easily affixed on the glass surface etc. .
  • A-1. 1 is a schematic cross-sectional view of a light control device according to one embodiment of the present invention.
  • the light control element 100a shown in FIG. 1 is an electric field drive type light control element, and includes a glass film 10, a light control layer 20, a resin film 30, and an adhesive layer 40 in this order.
  • the light control element 100 a further includes transparent electrode layers 50 a and 50 b for applying a voltage to the light control layer 20 between the glass film 10 and the light control layer 20 and between the light control layer 20 and the resin film 30.
  • the light control layer 20 includes, for example, a liquid crystal compound or an electrochromic material.
  • FIG. 2 is a schematic cross-sectional view of a light control device according to another embodiment of the present invention.
  • a dimming element 100b shown in FIG. 2 is a gaschromic dimming element, and includes a glass film 10, a dimming layer 20, a resin film 30, and an adhesive layer 40 in this order.
  • the light control element 100b has the space
  • the spacer 60 may be omitted as long as a space for introducing the gas is secured.
  • the light control layer 20 includes a gas chromic material.
  • the light control device of the present invention may be a light control device of a different system (for example, thermochromic system, photochromic system) from the illustrated example.
  • the peeling film may be laminated
  • the thickness of the light control element is, for example, 70 ⁇ m to 500 ⁇ m, preferably 80 ⁇ m to 450 ⁇ m, more preferably 100 ⁇ m to 400 ⁇ m, and further preferably 140 ⁇ m to 400 ⁇ m. .
  • the bending radius of the light control element is, for example, 20 mm to 100 mm, preferably 20 mm to 90 mm, and more preferably 20 mm to 80 mm. Since the light control element which has the bending radius in the said range is excellent in flexibility, it can wind in a roll shape and can form a film roll. Moreover, workability
  • A-2. Glass film Any appropriate glass film can be adopted. Examples of the glass constituting the glass film include soda-lime glass, borate glass, aluminosilicate glass, and quartz glass according to the classification by composition. Moreover, according to the classification
  • the content of alkali metal components (for example, Na 2 O, K 2 O, Li 2 O) in the glass is preferably 15% by weight or less, and more preferably 10% by weight or less.
  • the total light transmittance of the glass film is, for example, 80% or more, preferably 85% or more, and more preferably 90% or more.
  • the thickness of the glass film is, for example, 50 ⁇ m to 200 ⁇ m, preferably 50 ⁇ m to 180 ⁇ m. If the thickness of the glass film is less than 50 ⁇ m, the impact resistance may be insufficient. On the other hand, if the thickness of the glass film exceeds 200 ⁇ m, the flexibility decreases, and the weight increases, so that the workability when affixing to the glass surface or the like can be decreased.
  • thermoplastic resin examples include polyester resins such as PET; cycloolefin resins such as polynorbornene; acrylic resins; polycarbonate resins; and cellulose resins. Of these, polyester resins, cycloolefin resins, and acrylic resins are preferable. These resins are excellent in transparency, mechanical strength, thermal stability, moisture shielding properties and the like. You may use the said thermoplastic resin individually or in combination of 2 or more types. Moreover, it is also possible to use an optical film used for a polarizing plate, for example, a low retardation substrate, a high retardation substrate, a retardation plate, a brightness enhancement film, and the like.
  • the elastic modulus (tensile elastic modulus) at 23 ° C. of the resin film is preferably 2 GPa to 10 GPa, preferably 2 GPa to 6 GPa. According to the resin film having an elastic modulus within the above range, a highly brittle glass material is favorably supported, and as a result, a light control element having excellent flexibility can be obtained.
  • the thickness of the resin film is preferably 20 ⁇ m to 200 ⁇ m, more preferably 30 ⁇ m to 200 ⁇ m, and even more preferably 30 ⁇ m to 150 ⁇ m. According to the resin film having a thickness within the above range, a highly brittle glass material can be favorably supported, and the thickness of the light control element can be reduced, so that a light control element having excellent flexibility can be obtained.
  • the total light transmittance of the resin film is preferably 60% or more, more preferably 70% or more, and further preferably 80% or more.
  • Light control layer A-4-1 Light control layer containing a liquid crystal compound
  • the light control layer containing a liquid crystal compound is typically constituted by dispersing a liquid crystal compound in a polymer matrix. In the light control layer, it is possible to switch between the light transmission state and the light scattering state by changing the orientation degree of the liquid crystal compound depending on the presence or absence of voltage application.
  • the light control layer is in a light transmission state when a voltage is applied, and is in a light scattering state when no voltage is applied (normal mode).
  • the liquid crystal compound when the voltage is not applied, the liquid crystal compound is not oriented, so that the light scattering state occurs.
  • the liquid crystal compound is oriented so that the refractive index of the liquid crystal compound and the refractive index of the polymer matrix are As a result, the light transmission state is obtained.
  • the light control layer enters a light scattering state when a voltage is applied, and enters a light transmission state when no voltage is applied (reverse mode).
  • the alignment film provided on the surface of the transparent electrode layer aligns the liquid crystal compound when no voltage is applied and enters a light transmission state, and the application of the voltage disturbs the alignment of the liquid crystal compound and causes a light scattering state.
  • Examples of the light control layer as described above include a light control layer including a polymer dispersed liquid crystal, a light control layer including a polymer network type liquid crystal, and the like.
  • the polymer-dispersed liquid crystal has a structure in which liquid crystal compounds in the form of droplets are dispersed in a polymer matrix.
  • the polymer network type liquid crystal has a structure in which a liquid crystal compound is dispersed in a polymer network, and the liquid crystal in the polymer network has a continuous phase.
  • any appropriate non-polymerizable liquid crystal compound is used as the liquid crystal compound.
  • the dielectric anisotropy of the liquid crystal compound may be positive or negative.
  • the liquid crystal compound can be, for example, a nematic type, a smectic type, or a cholesteric type liquid crystal compound. It is preferable to use a nematic liquid crystal compound because excellent transparency can be realized in a light transmission state.
  • nematic liquid crystal compounds examples include biphenyl compounds, phenylbenzoate compounds, cyclohexylbenzene compounds, azoxybenzene compounds, azobenzene compounds, azomethine compounds, terphenyl compounds, biphenylbenzoate compounds, cyclohexylbiphenyl compounds. , Phenylpyridine compounds, cyclohexylpyrimidine compounds, cholesterol compounds, fluorine compounds, and the like.
  • the content of the liquid crystal compound in the light control layer is, for example, 40% by weight or more, preferably 50% by weight to 99% by weight, and more preferably 50% by weight to 95% by weight.
  • the resin forming the polymer matrix can be appropriately selected according to the light transmittance, the refractive index of the liquid crystal compound, and the like. It may be a light isotropic resin or a light anisotropic resin.
  • the resin is an active energy ray curable resin, for example, a liquid crystal polymer obtained by curing a polymerizable liquid crystal compound, a (meth) acrylic resin, a silicone resin, an epoxy resin, a fluorine resin. Resins, polyester resins, polyimide resins and the like can be preferably used.
  • the content of the polymer matrix in the light control layer is preferably 1% by weight to 60% by weight, and more preferably 5% by weight to 50% by weight.
  • the content of the polymer matrix is less than 1% by weight, problems such as low adhesion to the transparent conductive film may occur.
  • problems such as an increase in driving voltage and a dimming function may occur.
  • the thickness of the light control layer can be, for example, 10 ⁇ m to 100 ⁇ m, preferably 15 ⁇ m to 60 ⁇ m.
  • FIG. 3 is a schematic cross-sectional view of an example of a light control layer including an electrochromic material that can be used in the present invention.
  • the light control layer 20a containing an electrochromic material includes a first electrochromic compound layer 21 (first EC layer), an electrolyte layer 22, and a second electrochromic compound layer 23 (second EC layer) in this order.
  • the thickness of the light control layer 20a is, for example, 0.1 ⁇ m to 400 ⁇ m, preferably 0.5 ⁇ m to 200 ⁇ m.
  • the first EC layer is a dimming layer that changes its light transmittance and color according to the current flowing in the first EC layer together with the second EC layer described later.
  • the electrochromic compound for forming the first EC layer is not limited.
  • inorganic electrochromic such as tungsten oxide (for example, WO 3 ), molybdenum oxide, vanadium oxide, indium oxide, iridium oxide, nickel oxide, Prussian blue, etc.
  • Compounds for example, organic electrochromic compounds such as phthalocyanine compounds, styryl compounds, viologen compounds, polypyrrole, polyaniline, polythiophene (for example, poly (ethylenedioxythiophene) -poly (styrenesulfonic acid)), etc.
  • tungsten oxide and polythiophene are used.
  • the thickness of the first EC layer 10 is, for example, 0.01 ⁇ m or more, preferably 0.05 ⁇ m or more, and for example, 40 ⁇ m or less, preferably 20 ⁇ m or less.
  • the electrolyte layer is a layer for efficiently energizing the electrochromic compound inside the first EC layer and the second EC layer.
  • the electrolyte layer may be formed from a liquid electrolyte and a sealing material that seals the liquid electrolyte, or may be formed from a solid electrolyte membrane.
  • the electrolyte that forms the electrolyte layer is not limited.
  • LiClO 4 , LiBF 4 , LiAsF 6 , LiPF 6 , LiCF 3 SO 3 , LiCF 3 COO, KCl, NaClO 3 , NaCl, NaBF 4 , NaSCN, KBF 4 examples thereof include alkali metal salts or alkaline earth metal salts such as Mg (ClO 4 ) 2 and Mg (BF 4 ) 2 .
  • a quaternary ammonium salt, a quaternary phosphonium salt, etc. are mentioned.
  • an organic solvent is preferably used together with the electrolyte.
  • the organic solvent is not limited as long as it can dissolve the electrolyte, carbonates such as ethylene carbonate, propylene carbonate, and methyl carbonate; for example, furans such as tetrahydrofuran; for example, ⁇ -butyrolactone, 1,2-dimethoxyethane, Examples include 1,3-dioxolane, 4-methyl-1,3-dioxolane, methyl formate, methyl acetate, methyl propionate, acetonitrile, propylene carbonate, N, N-dimethylformamide and the like.
  • the electrolyte layer is preferably an electrolyte membrane containing an electrolyte, an organic solvent, and a binder resin.
  • Such an electrolyte layer can be obtained, for example, by mixing an electrolyte solution in which an electrolyte is dissolved in an organic solvent and a binder resin, and drying.
  • binder resin examples include acrylic resins such as polymethyl methacrylate.
  • the thickness of the electrolyte layer is, for example, 0.01 ⁇ m or more, preferably 0.1 ⁇ m or more, and for example, 300 ⁇ m or less, preferably 100 ⁇ m or less.
  • the same explanation as the first EC layer can be applied to the second EC layer.
  • the second EC layer may have the same configuration as the first EC layer or a different configuration.
  • FIG. 4 is a schematic cross-sectional view of an example of a light control layer containing a gas chromic material that can be used in the present invention.
  • the light control layer 20 b containing a gas chromic material includes a gas chromic compound layer 25 (GC layer) and a catalyst layer 26.
  • the light control layer 20b containing the gas chromic material is typically disposed so that the catalyst layer 26 is in contact with the gas (on the gap side).
  • the GC layer includes a chromic material whose state reversibly changes between a transparent state by hydrogenation and a reflection state by dehydrogenation.
  • the chromic material constituting the GC layer include rare earth metals such as Y, La, Gd and Sm, alloys of rare earth metals and magnesium, alloys of alkaline earth metals such as Ca, Sr and Ba, magnesium, Ni, Examples include alloys of transition metals such as Mn, Co, and Fe and magnesium.
  • the GC layer preferably contains magnesium because of its excellent transparency during hydrogenation, and a rare earth metal element-magnesium alloy is more preferred from the viewpoint of achieving both transparency and durability. Note that the GC layer may contain an element other than the alloy as a trace component.
  • the above metal or alloy constituting the GC layer contains a metal element that becomes transparent by hydrogenation and becomes reflective by releasing hydrogen.
  • a metal element that becomes transparent by hydrogenation and becomes reflective by releasing hydrogen For example, magnesium becomes transparent MgH 2 when hydrogenated, and becomes Mg having metal reflection by dehydrogenation.
  • the thickness of the GC layer is not particularly limited, but is preferably 10 nm to 500 nm, more preferably 15 nm to 200 nm, and more preferably 20 nm from the viewpoint of achieving both the light transmittance in the transparent state and the light shielding rate (reflectance) in the reflective state. More preferably, it is ⁇ 100 nm. If the thickness of the GC layer is excessively small, the light reflectance in the reflective state tends to be low. Moreover, when the film thickness of the GC layer is excessively large, the light transmittance in a transparent state tends to be low.
  • the catalyst layer has a function of promoting the hydrogenation and dehydrogenation of the GC layer.
  • the material of the catalyst layer is not particularly limited as long as it has a function of promoting hydrogenation and dehydrogenation of the GC layer.
  • the catalyst layer is selected from palladium, platinum, a palladium alloy, and a platinum alloy. It is preferred to have at least one metal.
  • palladium is preferably used because of its high hydrogen permeability.
  • the film thickness of the catalyst layer can be appropriately set depending on the reactivity of the GC layer, the catalyst capacity of the catalyst layer, and the like.
  • the film thickness of the catalyst layer is, for example, 1 nm to 30 nm, preferably 2 nm to 20 nm. If the thickness of the catalyst layer is excessively small, the hydrogenation and dehydrogenation catalytic functions may not be sufficiently exhibited. Moreover, when the film thickness of a catalyst layer is too large, there exists a tendency for light transmittance to fall.
  • the GC layer and the catalyst layer can be sequentially formed on the resin film by sputtering.
  • the light control layer 20b containing a gas chromic material may further include layers other than the GC layer 25 and the catalyst layer 26 as necessary.
  • a base layer may be provided on the side of the GC layer where the catalyst layer is not provided (for example, between the resin film and the GC layer), or a buffer layer may be provided between the GC layer and the catalyst layer.
  • a surface layer may be provided on the catalyst layer.
  • an inorganic oxide layer As a base layer between the resin film and the GC layer, moisture, oxygen gas, etc. generated from the resin film can be blocked and oxidation of the GC layer can be suppressed.
  • a metal thin film made of Ti, Nb, V, or an alloy of these metals as a buffer layer between the GC layer and the catalyst layer, migration of magnesium and the like from the GC layer to the catalyst layer is suppressed.
  • the switching speed from the transparent state to the reflective state due to dehydrogenation tends to increase.
  • the surface layer may have a function of blocking permeation of water and oxygen and preventing oxidation of the GC layer.
  • the material constituting the surface layer include inorganic materials such as inorganic oxides, organic materials such as polymers, and organic-inorganic hybrid materials.
  • the transparent electrode layer transparent electrode layer such as indium tin oxide (ITO), zinc oxide (ZnO), may be formed using a metal oxide such as tin oxide (SnO 2).
  • the first transparent electrode layer can be formed of a metal nanowire such as silver nanowire (AgNW), a carbon nanotube (CNT), an organic conductive film, a metal layer, or a laminate thereof.
  • the first transparent electrode layer can be patterned into a desired shape according to the purpose.
  • the total light transmittance of the transparent electrode layer is preferably 80% or more, more preferably 85% or more, and further preferably 90% or more.
  • the surface resistance value of the transparent electrode layer is preferably 0.1 ⁇ / ⁇ to 1000 ⁇ / ⁇ , more preferably 0.5 ⁇ / ⁇ to 500 ⁇ / ⁇ , and further preferably 1 ⁇ / ⁇ to 250 ⁇ / ⁇ . .
  • the thickness of the transparent electrode layer is preferably 0.01 ⁇ m to 0.06 ⁇ m, more preferably 0.01 ⁇ m to 0.045 ⁇ m. If it is such a range, the electrode layer excellent in electroconductivity and light transmittance can be obtained.
  • the transparent electrode layer can be provided on a glass film or a resin film using a method such as sputtering.
  • the transparent electrode layer may be directly formed on these films, and may be formed via a refractive index adjusting layer, a supporting base material, etc. as needed.
  • Adhesive layer Any appropriate adhesive composition can be used as the adhesive composition constituting the adhesive layer.
  • Specific examples of usable pressure-sensitive adhesive compositions include pressure-sensitive adhesive compositions based on (meth) acrylic polymers, silicone-based polymers, polyesters, polyurethanes, polyamides, polyethers, fluorine-based polymers, rubber-based polymers, and the like. Is mentioned. Among these, from the viewpoints of transparency, weather resistance, heat resistance and the like, an acrylic pressure-sensitive adhesive composition having an acrylic polymer as a base polymer is preferable.
  • the pressure-sensitive adhesive composition may further contain any appropriate additive as required.
  • the additive include a crosslinking agent, a tackifier, a plasticizer, a pigment, a dye, a filler, an anti-aging agent, a conductive material, an ultraviolet absorber, a light stabilizer, a release modifier, a softener, and a surfactant. , Flame retardants, antioxidants and the like.
  • crosslinking agent isocyanate crosslinking agent, epoxy crosslinking agent, peroxide crosslinking agent, melamine crosslinking agent, urea crosslinking agent, metal alkoxide crosslinking agent, metal chelate crosslinking agent, metal salt crosslinking agent, A carbodiimide type crosslinking agent, an oxazoline type crosslinking agent, an aziridine type crosslinking agent, an amine type crosslinking agent, etc. are mentioned.
  • the elastic modulus (storage elastic modulus) at 23 ° C. of the pressure-sensitive adhesive layer is preferably 1 ⁇ 10 ⁇ 5 GPa to 1 ⁇ 10 ⁇ 2 GPa, more preferably 5.0 ⁇ 10 ⁇ 5 GPa to 5.0 ⁇ 10 ⁇ . It can be 3 GPa, more preferably 1.0 ⁇ 10 ⁇ 4 GPa to 1.0 ⁇ 10 ⁇ 3 GPa.
  • the pressure-sensitive adhesive layer having such an elastic modulus can contribute to improvement in impact resistance and workability at the time of attachment. Moreover, when it has an adhesive layer which has such an elasticity modulus, when a long light control element is wound in roll shape, it can function as an impact relaxation layer.
  • the thickness (dry film thickness) of the pressure-sensitive adhesive layer is determined according to the desired pressure-sensitive adhesive force (peeling force).
  • the thickness (dry film thickness) of the pressure-sensitive adhesive layer is preferably about 20 ⁇ m to 200 ⁇ m, more preferably 20 ⁇ m to 150 ⁇ m, and still more preferably 25 ⁇ m to 100 ⁇ m.
  • the said light control element may be manufactured by arbitrary appropriate methods.
  • the light control film for example, unwinds a long resin film with a transparent electrode layer having a transparent electrode layer formed on one side in advance from a roll; while transporting the resin film with a transparent electrode layer in the longitudinal direction, Applying a composition for forming a light control layer on the surface of the transparent electrode layer to form a coating layer; a long glass film with a transparent electrode layer having a transparent electrode layer previously formed on one side of the coating layer; , Forming a laminate by continuously laminating the transparent electrode layer facing the coating layer and aligning the longitudinal direction of each other; obtaining the light control film by curing the coating layer A separately prepared long release film with a pressure-sensitive adhesive layer is continuously laminated so that the pressure-sensitive adhesive layer faces the resin film surface of the light control film and aligns
  • the composition for light control layer formation contains the monomer (preferably active energy ray hardening-type monomer) and liquid crystal compound for forming a polymer matrix, for example.
  • a glass roll with a light control layer in one embodiment of the present invention comprises a long glass film having a thickness of 50 ⁇ m to 200 ⁇ m, a light control layer laminated on one side of the glass film, Have.
  • the glass roll with a light control layer has a glass film, a light control layer, a resin film, and an adhesive layer in this order.
  • the glass film, the light control layer, the resin film, and the pressure-sensitive adhesive layer those described in the section A are preferably used.
  • the glass roll with a light control layer may be one in which the light control element described in the section A formed in a long shape is wound into a roll shape.
  • the above-mentioned glass roll with a light control layer is lightweight and has high reliability (impact resistance, scratch resistance, etc.), and when it has an adhesive layer, it can be easily attached to the glass surface or the like.
  • ⁇ Measurement method of elastic modulus> (Elastic modulus of resin film) A strip sample having a thickness of 50 ⁇ m, a width of 2 cm, and a length of 15 cm was prepared, and the elastic modulus was measured from the elongation and stress in the longitudinal direction of the strip sample using an autograph (manufactured by Shimadzu Corporation, AG-I). The test conditions were a distance between chucks of 10 cm and a pulling speed of 10 mm / min. (Elastic modulus of adhesive) The storage elastic modulus at 23 ° C. of the pressure-sensitive adhesive layer was measured using a viscoelasticity measuring device ARES (manufactured by TA Instruments).
  • ARES viscoelasticity measuring device
  • the pressure-sensitive adhesive layer was formed into a sheet having a thickness of 2 mm, punched out according to a parallel plate having a diameter of 25 mm, and attached to the chuck of the apparatus. Then, while applying strain at a period of 1 Hz, the temperature was increased from ⁇ 70 ° C. to 150 ° C. at a rate of temperature increase of 5 ° C./min, and the storage elastic modulus at 23 ° C. was measured. ⁇ Method for measuring thickness> Measurement was performed using a dial gauge.
  • the acrylic polymer solution was prepared by carrying out the polymerization reaction for 10 hours.
  • To 100 parts by weight of the solid content of the acrylic polymer solution 0.5 part by weight of an adduct of trimethylolpropane / tolylene diisocyanate (Nihon Polyurethane Kogyo Co., Ltd., Coronate L) as an isocyanate crosslinking agent, and a silane coupling agent ( 0.1 parts by weight of Shin-Etsu Chemical Co., Ltd. KBM403) was uniformly mixed and stirred to obtain an acrylic pressure-sensitive adhesive composition A.
  • a transparent electrode layer is formed by sputtering on one side of a transparent PET base material (Mitsubishi Chemical Co., Ltd., “Diafoil”, thickness: 188 ⁇ m, elastic modulus: 4.0 GPa) to obtain a PET film with an electrode layer It was.
  • a transparent electrode layer (ITO layer) was formed on one side of a glass film (Nippon Electric Glass Co., Ltd., “OA-10G”, thickness: 150 ⁇ m) by sputtering to obtain a glass film with an electrode layer.
  • a release film with a pressure-sensitive adhesive layer was obtained by applying the pressure-sensitive adhesive composition A to a release-treated surface of a PET film that had been subjected to a release treatment on one side, and drying it.
  • the pressure-sensitive adhesive layer had a thickness of 50 ⁇ m and an elastic modulus of 4 ⁇ 10 ⁇ 4 GPa.
  • a light control layer comprising a PET film with an electrode layer and a glass film with an electrode layer, comprising nematic liquid crystal molecules and 1,6-hexanediol diacrylate (manufactured by Nippon Kayaku Co., Ltd., “HDDA”) )
  • the polymer-dispersed liquid crystal layer forming composition was cured to obtain a laminate.
  • the said peeling film with an adhesive layer was laminated
  • a light control device having a configuration of [glass film / transparent electrode layer / light control layer / transparent electrode layer / resin film / adhesive layer / release film] was obtained.
  • the thickness from the glass film to the pressure-sensitive adhesive layer was 408 ⁇ m.
  • Example 2 A transparent PET substrate (“Diafoil”, thickness: 50 ⁇ m, elastic modulus: 4.0 GPa) manufactured by Mitsubishi Chemical Corporation was used as the resin film, and a glass film (manufactured by Nippon Electric Glass Co., Ltd., “ OA-10G ”(thickness: 100 ⁇ m) was used in the same manner as in Example 1 except that [glass film / transparent electrode layer / light control layer / transparent electrode layer / resin film / adhesive layer / release film] The light control element which has a structure was obtained. The thickness from the glass film to the pressure-sensitive adhesive layer was 220 ⁇ m.
  • Example 3 A transparent PET substrate (“Diafoil”, manufactured by Mitsubishi Chemical Corporation, thickness: 50 ⁇ m, elastic modulus: 4.0 GPa) was used as the resin film, and a glass film (manufactured by Nippon Electric Glass Co., Ltd., “OA-”). 10G ", thickness: 70 ⁇ m), and the thickness of the pressure-sensitive adhesive layer was changed to 20 ⁇ m, in the same manner as in Example 1, [Glass film / transparent electrode layer / light control layer / transparent electrode layer / A light control element having a structure of “resin film / adhesive layer / release film” was obtained. The thickness from the glass film to the pressure-sensitive adhesive layer was 160 ⁇ m.
  • Example 1 [Glass film / transparent electrode layer / light control layer / transparent] In the same manner as in Example 1 except that a glass film (manufactured by Nippon Electric Glass Co., Ltd., “OA-10G”, thickness: 300 ⁇ m) was used as the glass film.
  • the light control element which has the structure of an electrode layer / resin film / adhesive layer / release film] was obtained.
  • the thickness from the glass film to the pressure-sensitive adhesive layer was 558 ⁇ m.
  • a transparent PET substrate (Made by Mitsubishi Chemical, “Diafoil”, thickness: 50 ⁇ m, elastic modulus: 4.0 GPa) was used as the resin film, and a transparent PET substrate (Mitsubishi Chemical Corporation, “ [Diafoil], thickness: 100 ⁇ m), and the thickness of the pressure-sensitive adhesive layer was changed to 20 ⁇ m, in the same manner as in Example 1, [first resin film / transparent electrode layer / light control layer / A light control device having a configuration of transparent electrode layer / second resin film / adhesive layer / release film] was obtained. The thickness from the first resin film to the pressure-sensitive adhesive layer was 190 ⁇ m.
  • Example 3 A transparent PET base material (manufactured by Mitsubishi Chemical Corporation, “Diafoil”, thickness: 300 ⁇ m, elastic modulus: 4.0 GPa) was used as the resin film, and a glass film (manufactured by Nippon Electric Glass Co., Ltd., “ OA-10G ”(thickness: 100 ⁇ m) was used in the same manner as in Example 1 except that [glass film / transparent electrode layer / light control layer / transparent electrode layer / resin film / adhesive layer / release film] The light control element which has a structure was obtained. The thickness from the glass film to the pressure-sensitive adhesive layer was 470 ⁇ m.
  • a transparent PET substrate (“Diafoil”, thickness: 50 ⁇ m, elastic modulus: 4.0 GPa) manufactured by Mitsubishi Chemical Corporation was used as the resin film, and a glass film (manufactured by Nippon Electric Glass Co., Ltd., “ [Glass film / transparent electrode layer / light control layer / transparent electrode], in the same manner as in Example 1, except that OA-10G ”and thickness: 35 ⁇ m) were used, and the thickness of the pressure-sensitive adhesive layer was 20 ⁇ m.
  • the light control device of the example is good in both impact resistance and scratch resistance and has high reliability. Moreover, since the exposed surface when it affixes on a window etc. is a glass surface, it can be excellent also in durability. Furthermore, since it is lightweight and has an appropriate flexibility, the workability at the time of pasting was also excellent. On the other hand, the light control element of the comparative example has a problem in workability at the time of pasting as a result of either insufficient shock resistance or scratch resistance or insufficient flexibility. there were.
  • the present invention is suitably used in the field of light control films.

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  • Physics & Mathematics (AREA)
  • Nonlinear Science (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mathematical Physics (AREA)
  • Organic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Liquid Crystal (AREA)
  • Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
  • Surface Treatment Of Glass (AREA)
  • Glass Compositions (AREA)
  • Window Of Vehicle (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

La présente invention concerne un élément de gradation à poids modéré et à fiabilité élevée, pouvant facilement adhérer à une surface de verre ou à un support similaire. L'élément de gradation selon la présente invention est pourvu d'un film de verre, d'une couche de gradation, d'un film de résine et d'une couche adhésive, dans cet ordre, et a un rayon de cintrage de 20 à 100 mm, l'épaisseur dudit film de verre valant de 50 à 200 µm.
PCT/JP2019/011955 2018-03-28 2019-03-22 Élément de gradation comprenant un film de verre Ceased WO2019188736A1 (fr)

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CN201980021085.2A CN111902769B (zh) 2018-03-28 2019-03-22 包含玻璃膜的调光元件
EP19775974.9A EP3779577B1 (fr) 2018-03-28 2019-03-22 Élément de gradation comprenant un film de verre
JP2020509930A JP7274458B2 (ja) 2018-03-28 2019-03-22 ガラスフィルムを含む調光素子
KR1020207026079A KR102865558B1 (ko) 2018-03-28 2019-03-22 유리 필름을 포함하는 조광 소자
US16/979,633 US11143892B2 (en) 2018-03-28 2019-03-22 Dimming element including glass film

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JP7596897B2 (ja) 2021-03-31 2024-12-10 株式会社リコー エレクトロクロミック素子

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US11143892B2 (en) 2021-10-12
EP3779577A1 (fr) 2021-02-17
US20210026183A1 (en) 2021-01-28
JP7274458B2 (ja) 2023-05-16
TW201941946A (zh) 2019-11-01
TWI822743B (zh) 2023-11-21
CN111902769B (zh) 2024-07-02
EP3779577B1 (fr) 2024-10-23
CN111902769A (zh) 2020-11-06
KR102865558B1 (ko) 2025-09-26

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